Phase Equilibria in Ni-P-Sn

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Presentation transcript:

Phase Equilibria in Ni-P-Sn C. Schmetterer, J. Vizdal, H. Flandorfer and H. Ipser Department of Inorganic Chemistry – Materials Chemistry University of Vienna COST 531 Final Meeting, Vienna, May 2007

Technological Background Ni(P) layers as a contact material: Protective Ni-layer on Cu substrate in fact: amorphous Ni(P) layers; P is impurity! Interaction with Sn-based solders? basic information from phase diagram ternary phase diagram - and parts of the binaries! - have not yet been investigated

Binary Constituents Ni-Sn Phase Diagram P. Nash and A. Nash, Bull. Alloy Phase Diagrams, 6 (4) (1985) p. 350-358 C. Schmetterer et al., accepted for publication in Intermetallics

Ni-Sn Details Ni3Sn2 phase transition Ni3Sn phase transition

Ni-P and P-Sn both systems are currently under investigation experimental + CALPHAD

Sample Preparation from powders of binary end members (e.g. Ni3Sn) and red P, and Sn many problems! embrittlement of quartz capsules explosion of capsules samples contained in alumina crucibles alloyed in evacuated quartz tubes employing very slow heating, especially at P > 40 at.% annealed at 200, 550, 700, 850 and 1050 °C Ni2P Ni3Sn2 Ni3Sn

Investigations Short Term Scientific Mission host: A. Kodentsov, TUe In Vienna: DTA – not yet fully interpreted XRD – isothermal sections Short Term Scientific Mission host: A. Kodentsov, TUe Light microscopy + polarized light SEM / EDS diffusion couples

Phase relations at 550 °C Ternary phases: Ni2PSn Ni10P3Sn Ni10P3Sn5 T4 – new phase? Pseudo-binary System Ni2P – Sn?

Phase relations at 700 °C

Phase relations at 850 °C

Diffusion Couples

Diffusion Couples Ni3Sn / Ni2P Annealed at 700 °C in vacuum for 100 h ?? Ni3Sn Ni12P5 100 µm

Diffusion Couples Sn / Ni2P Annealed at 200 °C in vacuum for 4 months Ni2PSn Ni2P Sn

Conclusion and Outlook Ni-P-Sn: first information on phase equilibria diffusion couples Planned investigations: continue the phase diagram study Calorimetry – enthalpy of mixing, enthalpy of formation CALPHAD study of the system

Thank You for Your Attention Acknowledgements Thanks to: K. Richter, U. Saeed A. Kodentsov (TU Eindhoven, NL) H. Schmidt (Dep. f. Physical Chemistry) P. Roussel (Ecole Nationale Superieure de Lille) A. Leineweber (MPI Stuttgart) FWF P-16495-N11, COST 531, ELFNET Thank You for Your Attention

Ni3Sn Phases – Crystal Structures Ni3Sn LT: hexagonal – O.K. Ni3Sn HT: quenching > 2000°C/sec. : martensitic transformation to orthohombic bCu3Ti structure (Pak) Bull. Jpn. Inst. Met., 37(10) (1973) p. 1128-1134) Thermodyn. stable HT phase is cubic with BiF3 type structure (Schubert; Naturwissenschaften, 43 (1956) p. 248) only found in powders quenched from 1050 °C Otherwise massive transformation to LT phase

Ni3Sn2 Phase Region crystallographic relation between NiAs-type HT-phase and the three orthorhombic LT-phases *) thermal effects detected by heat-flow DSC transitions involve four invariant reactions *) incommensurate LT‘ and LT‘‘: A. Leineweber, Journal of Solid State Chemistry, 159 (2001) p. 191-197 and Journal of Solid State Chemistry, 177 (2004) p. 936-945 and p. 1197-1212